Blue diphenylnaphthylmethane dye.



UNITED STATES PATENT OFFICE.

ARTHUR HAUSDDRFER AND FRIEDRICH REINGRUBER, OF ELBERFELD, GERMANY,ASSIGNORS TO THE FARBENFABRIKEN OF ELBERFELD COMPANY, OF NEW YORK.

BLUE D IPHENY LNAPHTHYLM ETHANE DYE.

SPECIFICATION forming part of Letters Patent No. 647,260, dated April10, 1900.

Application filed Jam ie, 1900.

To all whom, it may concern:

Be it known that we, ARTHUR I-IAUsDoRnER and FRIEDRICH REINGRUBER,doctors of philosophy, chemists, (assignors to the FAR- BENFABRIKEN orELBERFELD COMPANY, on NEW YORK,) residing at Elberfeld, Germany, haveinvented a new and useful Improvement in Blue DiphenylnaphthylmethaneDye; and we hereby declare the following to be a clear and exactdescription of our invention.

We havefound that valuable new dyestuifs capable of dyeing wool inacid-baths blue shades are obtained if basic dyestuffs of the so-calledVictoria-blue series hav- .ing the general formula (R meaning an alkylradical such as methyl, ethyl, or the like, R meaning an alkyl radicalsuch as methyl, ethyl, phenyl, paratolyl, or the like) are treated in asuitable manner with sulfonating agents.

The new dyestuff sulfonic acids represent, when dry and pulverized,brown powders soluble in water With a blue color and dyeing unmordantedwool in acid-baths very clear and even blue shades. V

In carrying out our new process practically we can proceed as follows,the parts being, by Weight: twenty parts of the carefully dried andpulverized dyestuff obtainable by condensingtetramethyldiamidobenzophenone Serial No. 1,658. (No specimens.)

with paratolylalphanaphthylamin in the presence of phosphorus oxychloridare dissolved in one hundred parts of sulfuric monohydrate while beingcooled and stirred. To the solution thus produced thirty-six parts offuming sulfuric acid (containing seventy per cent. of 80,) are addedwhile continuously stirring, the temperature being kept below zero. Themixture thus obtained is allowed to stand for some time at from 0 to 5centigrade until a test portion poured into water dissolves completelyin hotdilute alkalies. The mixture is then immediately poured on ice andis neutralized with sodium carbonate, by means of which operation thedyestufi is precipitated. Finally the dyestuff is isolated byfiltration. It can be further purified in the known manner by dissolvingthe same in hot water and precipitating again from the resultingsolution by the addition of common salt.

The new coloring-matter thus produced represents when dry and pulverizeda brown powder soluble in water with a blue color. It is soluble inalcohol with a blue color; in glacial acetic acid with a greenish-bluecolor. In concentrated sulfuric acid (of 66 Baum) it dissolves with adarkred color, which changes into brown on the additionof a smallquantity of ice, while the color is changed first into grayish green andthen into grayish blue on the addition of a larger quantity of ice, adark-brown precipitate being at the same time separated. The newdyestuff yields on Wool in acid-baths beautiful blue, clear, and evenshades. Very similar results are obtained if other of the above-definedbasic dyestuffs are employed in the foregoing example.

Having now described our invention and in what manner the same is to beperformed, what We claim as new, and desire to secure by Letters Patent,is-

1. The process for producing new diphenylnaphthylmethane dyestuffs whichprocess consists in first acting with fuming sulfuric acid on basicdyestuffs of the general formula:

and secondly isolating the dyestuff sulfonic acid thus obtained in theform of an alkaline salt, substantially as hereinbefore described.

3. As new articles of manufacture the new dyestuffs of thediphenylnaphthylmethane series being when dry and pulverized brownpowders, soluble in water and in alcohol with a blue color, dyeing woolin acid-baths blue shades, substantially as hereinbefore described.

4. Asa new article of manufacture the new dyestuif of thediphenylnaphthylmethane series obtained from the basic coloring-matterof the formula:

being when dry and pulverized a brown powder, soluble in water and inalcohol with a blue color,in glacial acetic acid with a greenish-bluecolor, being dissolved by concentrated sulfuric acid with a dark-redcolor which changes into brown on the addition of a small quantity ofice while the color is changed first into grayish, green and then intograyish blue on the addition of a larger quantity of ice a dark-brownprecipitate being at the same time precipitated, dyeing wool inacid-baths beautiful blue, clear and even shades, substantially ashereinbefore described.

In testimony whereof wehave signed our names in the presence of twosubscribing witnesses.

ARTHUR HAUSDORFER. FRIEDRICH REINGRUBER. \Vitnesses:

OTTO KoNIG, F. I. RITTERHAUS.

